CN101164899B - Method for synthesizing non-aqueous system nano-crystal zirconium dioxide - Google Patents
Method for synthesizing non-aqueous system nano-crystal zirconium dioxide Download PDFInfo
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- CN101164899B CN101164899B CN2007101395501A CN200710139550A CN101164899B CN 101164899 B CN101164899 B CN 101164899B CN 2007101395501 A CN2007101395501 A CN 2007101395501A CN 200710139550 A CN200710139550 A CN 200710139550A CN 101164899 B CN101164899 B CN 101164899B
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- zirconium dioxide
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Abstract
This invention relates to a method for synthesizing non-aquo nanometer crystal zirconium dioxide. In this invention, C1-C4 organic acid (1) and zirconium isopropoxide (2) are used as raw materials with molar ratio of: (1):(2)=(2-10):1. After mixing, said mixture is put in a reactor, heating to 120-240deg.C for 10-24 hrs to obtain wet gel of zirconium dioxide, which is then washed by ethanol for 3-5 times, being dried under 100-160deg.C to obtain this inventive nanometer grade crystal zirconium dioxide product. This invention has advantages of: no aquo-system is needed for the whole production process, this inventive hydrolysis needs no control, simple process, convenient operation, mild reaction condition, high yield, no environmental pollution, high value of side-products, high crystallinity, high pureness and narrow particle size distribution.
Description
Technical field
The invention belongs to the preparation method of zirconium dioxide, specifically is exactly preparation crystalline nano zirconium dioxide in non-aqueous system.
Technical background
Zirconium dioxide is a kind of high temperature resistant, wear-resistant, corrosion-resistant, the ceramic with good optical, calorifics, electricity and mechanical properties.Nano level zirconium dioxide powder has particular performances especially, is down isolator as normal temperature, has electroconductibility, increasing tougheness and a sensitivity characteristic etc. and high temperature is next; Have at aspects such as pottery, rubber, coating, daily-use chemical industry, catalysis widely simultaneously and use.The degree of crystallinity of zirconium dioxide, purity and granularity are decision powder property and key in application factor.Therefore, research preparation high-crystallinity, high purity, nano level ZrO
2Significant, become that present scientific worker pays close attention to and the focus of research.
The preparation method of zirconium dioxide is a lot, comprises hydrothermal method, microwave-hydrothermal method, sol-gel method and coprecipitation method etc., but these methods or owing to will control the hydrolysis of zirconium precursor body, the preparation process complexity, the reaction times is longer; Or the ZrO that obtains
2Be unbodied powder, need just can obtain the ZrO of advantages of good crystallization through high-temperature post-treatment
2
Summary of the invention
The object of the invention provides that a kind of technology is simple, easy and simple to handle, the nanometer ZrO of advantages of good crystallization
2Synthetic method.
The object of the present invention is achieved like this: utilize the presoma of zirconium and organic acid to be raw material, then reacting by heating for some time in reactor, just can obtain the good ZrO of crystallization after the oven dry
2
The inventive method is as follows:
It is raw material that the present invention adopts zirconium iso-propoxide and C1～C4 organic acid, the mol ratio of organic acid and zirconium iso-propoxide is 2～10: 1, be transferred in the reactor after the mixing, be prepared into the zirconium white wet gel in 10～24 hours 120～240 ℃ of processing, with the zirconium white wet gel with ethanol give a baby a bath on the third day after its birth～five times, dry under 100～160 ℃ condition again, can obtain crystalline nano level zirconium dioxide.
Aforesaid C1～C4 organic acid is formic acid, acetic acid, propionic acid, butanic acid, isopropylformic acid.
The present invention compared with prior art has following advantage:
1. whole process of preparation is carried out at non-aqueous system, and hydrolytic process does not need control;
2. technology is simple, easy and simple to handle, reaction conditions is gentle, productive rate is high;
3. react the by product environmentally safe that generates, secondary valence value height;
4. the product degree of crystallinity height that obtains, purity height, narrow diameter distribution.
Embodiment
Embodiment 1
Is to be transferred in the reactor after mixing at 2: 1 with formic acid and zirconium iso-propoxide with mol ratio, 140 ℃ of reactions 12 hours, reactant is given a baby a bath on the third day after its birth time with ethanol, then 100 ℃ of oven dry, promptly obtains crystalline zirconium dioxide material.
Embodiment 2
Is to be transferred in the reactor after mixing at 6: 1 with acetic acid and zirconium iso-propoxide with mol ratio, 200 ℃ of reactions 12 hours, reactant is washed five times with ethanol, then 100 ℃ of oven dry, promptly obtains crystalline zirconium dioxide material.
Embodiment 3
Is to be transferred in the reactor after mixing at 4: 1 with butanic acid and zirconium iso-propoxide with mol ratio, 220 ℃ of reactions 12 hours, reactant is washed four times with ethanol, then 120 ℃ of oven dry, promptly obtains crystalline zirconium dioxide material.
Embodiment 4
Is to be transferred in the reactor after mixing at 10: 1 with formic acid and zirconium iso-propoxide with mol ratio, 200 ℃ of reactions 12 hours, reactant is given a baby a bath on the third day after its birth time with ethanol, then 140 ℃ of oven dry, promptly obtains crystalline zirconium dioxide material.
Embodiment 5
Is to be transferred in the reactor after mixing at 4: 1 with acetic acid and zirconium iso-propoxide with mol ratio, 180 ℃ of reactions 16 hours, reactant is given a baby a bath on the third day after its birth time with ethanol, then 100 ℃ of oven dry, promptly obtains crystalline zirconium dioxide material.
Embodiment 6
Is to be transferred in the reactor after mixing at 4: 1 with propionic acid and zirconium iso-propoxide with mol ratio, 240 ℃ of reactions 12 hours, reactant is washed five times with ethanol, then 160 ℃ of oven dry, promptly obtains crystalline zirconium dioxide material.
Claims (1)
1. a non-aqueous system nano-crystal zirconium dioxide synthetic method is characterized in that comprising the steps:
Adopting zirconium iso-propoxide and C1～C4 organic acid is raw material, the mol ratio of organic acid and zirconium iso-propoxide is 2～10: 1, be transferred in the reactor after the mixing, be prepared into the zirconium white wet gel in 10～24 hours 120～240 ℃ of processing, with the zirconium white wet gel with ethanol give a baby a bath on the third day after its birth～five times, dry under 100～160 ℃ condition again, promptly obtain crystalline nano level zirconium dioxide;
Described C1～C4 organic acid is formic acid, acetic acid, propionic acid, butanic acid or isopropylformic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101395501A CN101164899B (en) | 2007-09-29 | 2007-09-29 | Method for synthesizing non-aqueous system nano-crystal zirconium dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101395501A CN101164899B (en) | 2007-09-29 | 2007-09-29 | Method for synthesizing non-aqueous system nano-crystal zirconium dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101164899A CN101164899A (en) | 2008-04-23 |
| CN101164899B true CN101164899B (en) | 2010-09-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101395501A Expired - Fee Related CN101164899B (en) | 2007-09-29 | 2007-09-29 | Method for synthesizing non-aqueous system nano-crystal zirconium dioxide |
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| CN (1) | CN101164899B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102180516B (en) * | 2011-03-15 | 2013-06-12 | 宣城晶瑞新材料有限公司 | Preparation method of non-hydrosol gel of high-dispersibility nano zirconia |
| CN109718738B (en) * | 2017-10-27 | 2022-08-12 | 中国石油化工股份有限公司 | Zirconia spherical adsorbent and preparation method and application thereof |
| CN109110809A (en) * | 2018-08-03 | 2019-01-01 | 长江大学 | A kind of composite cathode material for lithium ion cell ZrO2And preparation method thereof |
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2007
- 2007-09-29 CN CN2007101395501A patent/CN101164899B/en not_active Expired - Fee Related
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| CN101164899A (en) | 2008-04-23 |
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